Synthesis of PbTiO3 by use of polymeric precursors

Lead titanate powders were synthesized through the use of polymeric precursors according to the Pechini Process. The polymeric precursor was calcined at temperatures ranging from 300 to 600°C for 1 or 2 h. X-ray diffraction (XRD) showed that lead titanate crystallizes from the precursor at temperatures as low as 400°C. No intermediate carbonate phase was detected by Fourier transform infrared spectroscopy (FTIR) or by XRD. A powder with mean particle size of 150 nm was obtained after calcination of the precursor at 600°C for 1 h. © 1998 Elsevier Science B.V. All rights reserved.

Preparation and characterization of SrBi2Nb2O9 thin films made by polymeric precursors

A polymeric precursor solution was employed in preparing SrBi2Nb2O9 (SBN) powder and thin films dip coated onto Si(100) substrate. XRD results show that the SBN perovskite phase forms at temperatures as low as 600°C through an intermediate fluorite phase. This fluorite phase is observed for samples heat-treated at temperatures of 400 and 500°C. After heat treatment at temperatures ranging from 300 to 800°C, thin films were shown to be crack free. Grazing incident angle XRD characterization shows the occurrence of the fluorite intermediate phase for films also. The thickness of films, measured by MEV, was in the order of 80-100 nm.

Sulfur-containing palladacycles as catalyst precursors for the heck reaction

(formula presented) The air, water, and highly thermally stable sulfur-containing palladacycles, mainly derived from the ortho-palladation of benzylic thioethers, are exceptional catalyst precursors for the Heck reaction. The reaction can be performed with aryl iodides, bromides, and chlorides, with acrylic esters and styrene, leading to turnover numbers up to 1 850 000.

Sulfur-containing palladacycles: Efficient phosphine-free catalyst precursors for the Suzuki cross-coupling reaction at room temperature

Cyclopalladated compounds derived from the ortho-metalation of benzylic tert-butyl thioethers are excellent catalyst precursors for the Suzuki cross-coupling reaction of aryl bromides and chlorides with phenylboronic acid under mild reaction conditions. A broad range of substrates and functional groups are tolerated in this protocol, and highly catalytic activity is attained.

Preparation and characterization of BaBi2Nb2O9(BBN) ceramics synthetized by polymeric precursors method

Pure BBN powders and with addition of 1 and 2 wt% in excess of bismuth were obtained by Pechini Method. The powders calcined at 300°C/4h were analyzed by TG/DTA to study the temperature of organic matter decomposition. A systematic study of calcination temperature and time to the formation of the BBN phase was performed and the phase formation was accompanied by XRD. The calcined powders at 800°C during 2h were analyzed by infrared spectroscopy and by BET. The powders were isostaticaly pressed and sintered at temperatures ranging from 900°C to 1000°C. The ceramics were characterized by XRD to control the crystalline phase and by SEM to analyze the microstructure.

Effect of magnesium on the properties of LiNbO 3 thin films prepared from polymeric precursors

The effect of magnesium addition on the phase formation, microstructure and electric and ferroelectric properties of LiNbO 3 thin films prepared through polymeric precursors was analyzed. By X ray diffraction no secondary phase was observed with the increase of magnesium concentration. Comparing to pure LiNbO 3, the addition of 0.5 and 1.0 mol% of Mg +2 increased of the dielectric constant, while 2.0 mol% decreased it. It was noticed that the increase in additive concentration decreases the ferroelectric remanent polarization and increases the coercive field. © 2002 Taylor & Francis.

Microstructure of doped barium titanate prepared from polymeric precursors

Barium titanate is used extensively as a dielectric in ceramic capacitors, particularly due to its high dielectric constant and low dielectric loss characteristics. It can be made semiconducting by addition of certain dopants and by proper modification of grains and grain boundary properties obtaining very interesting characteristics for various applications. The synthesis method and sintering regime have a strong influence on properties of obtained barium titanate ceramics. Doped barium titanate was prepared with Nb+5 and Y+3 ions as donor dopants, and with Mn+2 ions as acceptor dopant by polymeric precursors method. By this procedure nanosized powders were obtained after calcination. Sintering was performed in the temperature range of 1290°C to 1380°C The microstructure of doped BaTiO3 was performed using scanning electron microscopy. The influence of dopants and sintering temperature on grain size was analysed.

Modelling study of the impact of deep convection on the utls air composition - Part I: Analysis of ozone precursors

The aim of this work is to study the local impact on the upper troposphere/lower stratosphere air composition of an extreme deep convective system. For this purpose, we performed a simulation of a convective cluster composed of many individual deep convective cells that occurred near Bauru (Brazil). The simulation is performed using the 3-D mesoscale model RAMS coupled on-line with a chemistry model. The comparisons with meteorological measurements show that the model produces meteorological fields generally consistent with the observations. The present paper (part I) is devoted to the analysis of the ozone precursors (CO, NO x and non-methane volatile organic compounds) and HO x in the UTLS. The simulation results show that the distribution of CO with altitude is closely related to the upward convective motions and consecutive outflow at the top of the convective cells leading to a bulge of CO between 7 km altitude and the tropopause (around 17km altitude). The model results for CO are consistent with satellite-borne measurements at 700 hPa. The simulation also indicates enhanced amounts of NO x up to 2 ppbv in the 7-17 km altitude layer mainly produced by the lightning associated with the intense convective activity. For insoluble non-methane volatile organic compounds, the convective activity tends to significantly increase their amount in the 7-17km layer by dynamical effects. During daytime in the presence of lightning NO x, this bulge is largely reduced in the upper part of the layer for reactive species (e.g. isoprene, ethene) because of their reactions with OH that is increased on average during daytime. Lightning NO x also impacts on the oxydizing capacity of the upper troposphere by reducing on average HO x, HO 2, H 2O 2 and organic hydroperoxides. During the simulation time, the impact of convection on the air composition of the lower stratosphere is negligible for all ozone precursors although several of the simulated convective cells nearly reach the tropopause. There is no significant transport from the upper troposphere to the lower stratosphere, the isentropic barrier not being crossed by convection. The impact of the increase of ozone precursors and HO x in the upper troposphere on the ozone budget in the LS is discussed in part II of this series of papers.

Electrical devices obtained from polymeric precursors process

Nowadays, many investments have been made in the area of superconductor materials, with the aim to improve their potential technological applications. Applications on the energy transport using cables, to get high resolution images in the medicine use high magnetic fields, high speed signals use superconductor devices all of them are in crescent evidence and they are showing that the future is coming and next for this new kind of materials. Obviously that everything of this is possible due to the increasing of research with new materials, where the synthesis, characterization and applications are of the mainly objective of these researches. The production of cable for the energy transport has been in advanced stage as the bulks production is too. However, the film production that to aim at the electronic devices area is not as developed or it still need expensive investments. Thinking about that, we are developing a research where we may increase the relation of cost/benefits. Thereby, we are applying the polymeric precursors method to obtain films that will be used in the built of electronic devices. Thin films (mono and multilayers, on crystalline or metallic substrates, controlled thickness) of the BSCCO system have been obtained from dip coating deposition process with excellent results in terms of preferential orientation, controlled thickness, a large area, which may indicate future applications. Based on these results, we present an electrical circuit and their principal characteristics as superconductor transition (85K), transport current density and structure. DC four probes method, scanning electron microscopy, digital optical microscopy and X-ray diffractometry were some techniques used for the characterization of this superconductor electric device. © 2006 Materials Research Society.

Heating rate and temperature effects on the BaTiO3 formation by thermal decomposition of (Ba,Ti) organic precursors during the Pechini process

Different thermal treatments for the synthesis of BaTiO3 powder obtained through the Pechini method were studied. The synthesis of BaTiO3 starts at 150 °C by the thermal dehydration of organic precursors. The usual inevitable formation of barium carbonate during the thermal decomposition of the precursor could be retarded at lower calcination temperatures and optimized heating rates. The organic precursors were treated at temperatures between 200 and 400 °C. Then, the samples were calcined at 700 and 800 °C for 4 and 2 h, respectively. The resulting ceramic powders were characterized by gravimetric and differential thermal analyses, X-ray powder diffraction and infrared spectroscopy. It was found that depending on the heating rate and final temperature of the thermal treatment, high amounts of BaCO3 and TiO2 could be present due to the high concentration of organics in the final calcination step. © 2007 Elsevier B.V. All rights reserved.

Comparison of the biological behavior of wollastonite bioceramics prepared from synthetic and natural precursors

Wollastonite bioceramics prepared from synthetic and natural precursors were implanted in rats in bone and subcutaneous tissues. The implant sites were excised after 7, 30 and 120 days, fixed, dehydrated, embedded in paraffin wax for serial cutting and examined under transmitted light microscope. It was found a very similar behavior for both wollastonite bioceramics. They were biocompatible, bioactive and biodegradable when implanted in rat bone. The synthetic ceramic was more reabsorbable than the one from natural powder. When implanted in subcutaneous rat tissue, both materials elicited a mild initial inflammatory reaction that practically disappeared after 120 days. Both materials were encapsulated with a very thin fibrous capsule and slightly reabsorbed at their surfaces. None of the materials induced ectopic osteogenesis. According to the results, the studied materials seem to be able for manufacturing reabsorbable bone implants.

Characterization of Zn0. 95Mn0.05O synthesized by polymeric precursors

This paper discusses the preparation and characterization of Zn 0.95Mn0.05O phase obtained by the polymeric precursor method for DMS applications. The as-obtained powders were calcined between 500 to 800°C and characterized by XRD, SEM and BET. The XRD analysis of the powder showed a crystalline material containing second phase. The crystallite sizes ranged from 20 to 51 nm. The micrographs showed that the powders consisted of soft and homogeneous agglomerations. The nitrogen adsorption/desorption curves of the Zn0.95Mn0.05O phases were type II curves, which is characteristic of mesoporous materials.

A study of the precursors and photoactivity of nanostructures of Ti oxides synthesized by the alkaline hydrothermal method

The present study describes the synthesis, characterization and photocatalytic potential of Ti oxide nanostructures of various morphologies and crystalline phases that were synthesized from 4 different precursors by the alkaline hydrothermal method. The materials were characterized by mainly X-ray diffraction (XRD), Raman spectroscopy, scanning and transmission electron microscopy (SEM and TEM), thermogravimetric analysis (TGA) and X-ray absorption spectroscopy (XAS). Also, photocatalytic potential was assessed by rhodamine B photodegradation. The materials obtained from peroxytitanium complexes (PTCs) exhibited a strong dependence on the concentration of KOH ([KOH]) used for synthesis. The pre-formed sheets of the PTCs were critical to the formation of nanostructures such as nanoribbons, and they were also compatible with the rolling up process, which can be utilized to form structures such as nanorods, nanowires or nanotubes. In the rhodamine photodegradation tests, TiO2 anatase nanostructures with six-coor inated Ti were more effective than the titanate ones (five-coordinated), despite having a smaller surface area and fewer OH groups. The lower photoactivity of the titanates was attributed to the presence of five-coordinated titanium species (TiO5), which may act as electron-hole recombination centers. Furthermore, the material with a mixture of TiO2/titanate was shown to be promising for photocatalytic applications. © 2013 by American Scientific Publishers.

Osteogenesis-inducing calcium phosphate nanoparticle precursors applied to titanium surfaces

This study investigated the effects of the morphology and physicochemical properties of calcium phosphate (CaP) nanoparticles on osteogenesis. Two types of CaP nanoparticles were compared, namely amorphous calcium phosphate (ACP) nano-spheres (diameter: 9-13 nm) and poorly crystalline apatite (PCA) nano-needles (30-50 nm x 2-4 nm) that closely resemble bone apatite. CaP particles were spin-coated onto titanium discs and implants; they were evaluated in cultured mouse calvarial osteoblasts, as well as after implantation in rabbit femurs. A significant dependence of CaP coatings was observed in osteoblast-related gene expression (Runx2, Col1a1 and Spp1). Specifically, the PCA group presented an up-regulation of the osteospecific genes, while the ACP group suppressed the Runx2 and Col1a1 expression when compared to blank titanium substrates. Both the ACP and PCA groups presented a more than three-fold increase of calcium deposition, as suggested by Alizarin red staining. The removal torque results implied a slight tendency in favour of the PCA group. Different forms of CaP nanostructures presented different biologic differences; the obtained information can be used to optimize surface coatings on biomaterials. © 2013 IOP Publishing Ltd.

Resistance training for explosive and maximal strength: Effects on early and late rate of force development

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)